Diazomethane → HCID 178497913, 화합물

HRID 487064노트

반응식

HRID 487064 반응식
[N+](=[CH2:3])=[N-].[OH:4][C:5]1[N:13]=[C:12]([CH3:14])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8]>CCOCC.C1COCC1>[OH:4][C:5]1[N:13]=[C:12]([CH3:14])[CH:11]=[CH:10][C:6]=1[C:7]([O:9][CH3:3])=[O:8]

참가 물질

5

반응물 2

HCID 9550DiazomethaneHCID 178425908HCID 178425908, 화합물

생성물 1

HCID 178497913HCID 178497913, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

Excess diazomethane in ether was added portionwise over 15 mins to 9.58 g (~60 mmoles) of 2-hydroxy-6-methyl nicotinic acid in 900 mL of THF at 0°. After stirring 2 hours, excess diazomethane was removed in vacuo. The resulting white solid was filtered and washed with hexane and dried. This fluffy solid was the required methyl ester. The filtrate was concentrated. The resulting solid was redissolved in a minimum amount of THF and hexane was added until no further precipitation was observed. Solid was filtered and washed with hexane and dried to provide more of the desired compound.

후처리

  1. customexcess diazomethane was removed in vacuo
  2. filtrationThe resulting white solid was filtered
  3. washwashed with hexane
  4. customdried
  5. concentrationThe filtrate was concentrated
  6. dissolutionThe resulting solid was redissolved in a minimum amount of THF and hexane
  7. additionwas added until no further precipitation
  8. filtrationSolid was filtered
  9. washwashed with hexane
  10. customdried

출처 및 근거

ORD 기록
ord-081eee156929442594546633c0e75235
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294610

반응 노트

불러오는 중…